CN110541153A - Method for preparing film by deposition and film coating machine - Google Patents

Method for preparing film by deposition and film coating machine Download PDF

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Publication number
CN110541153A
CN110541153A CN201810525968.4A CN201810525968A CN110541153A CN 110541153 A CN110541153 A CN 110541153A CN 201810525968 A CN201810525968 A CN 201810525968A CN 110541153 A CN110541153 A CN 110541153A
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metal film
sputtering
ion source
substrate
film
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李紫茵
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Individual
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    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/02Pretreatment of the material to be coated
    • C23C14/021Cleaning or etching treatments
    • C23C14/022Cleaning or etching treatments by means of bombardment with energetic particles or radiation
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14Metallic material, boron or silicon
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34Sputtering
    • C23C14/3435Applying energy to the substrate during sputtering
    • C23C14/3442Applying energy to the substrate during sputtering using an ion beam
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34Sputtering
    • C23C14/46Sputtering by ion beam produced by an external ion source

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physical Vapour Deposition (AREA)

Abstract

the invention discloses a method for preparing a film by deposition and a film coating machine, wherein the method comprises the following steps: preparing a substrate; in the process of sputtering and depositing the metal film on the surface of the substrate by adopting a sputtering ion source, an auxiliary ion source is adopted to bombard the metal film so as to enhance the surface mobility of atoms of the metal film and improve the compactness of the metal film. The method and the film coating machine provided by the invention solve the technical problem that the metal film with both high thickness and high density is difficult to prepare in the existing metal film preparation scheme, and provide the method and the film coating machine for generating the metal film with high thickness and high density.

Description

Method for preparing film by deposition and film coating machine
Technical Field
the invention relates to the technical field of metal film preparation, in particular to a method for preparing a film by deposition and a film coating machine.
Background
Metal films have many applications in both semiconductor devices and optical devices, and are used mainly to alter the path of light or to receive optical signals, such as transmitting telescopes, high efficiency light emitting diodes or space satellite reflectors.
At present, the main preparation methods of metal films include an electron gun evaporation technology and an ion beam sputtering coating technology, wherein a film with a columnar microstructure is obtained by the traditional electron gun evaporation technology, the stacking density of the film is about 0.7 at room temperature, and pores of the columnar structure in the film can adsorb water vapor in the atmosphere, so that the original refractive index and optical thickness are changed to influence the stability of the optical film, and thus, the higher the density of the metal film is, the better the optical stability is. In the conventional ion beam sputtering coating technology, taking aluminum film preparation as an example, high-energy ion beams generated by an Ar ion source bombard an aluminum target material placed in high vacuum, so that target material atoms are sputtered out and recombined on the surface of a substrate to form a thin film, and a metal film with higher density can be prepared by ion beam sputtering coating.
however, when a thick high-density metal film is required to be prepared, since the bonding force between the metal film and the substrate is often insufficient, even though the ion beam sputtering coating technology is adopted, the problem that the internal stress is large and the metal film is easy to crack exists, so that the metal film with high density and high thickness requirements is difficult to prepare.
therefore, the existing metal film preparation scheme has the technical problem that the metal film with both high thickness and high density is difficult to prepare.
Disclosure of Invention
The invention provides a method for preparing a film by deposition and a film coating machine, which solve the technical problem that the existing metal film preparation scheme is difficult to prepare a metal film with both high thickness and high density.
In one aspect, the present invention provides a method for depositing a prepared film, comprising:
Preparing a substrate;
and sputtering and depositing a metal film on the surface of the substrate by adopting a sputtering ion source, wherein in the process of sputtering and depositing the metal film on the surface of the substrate by adopting the sputtering ion source, an auxiliary ion source is adopted to bombard the metal film so as to enhance the surface mobility of metal film atoms and improve the compactness of the metal film.
optionally, the metal film is an aluminum film.
Optionally, in the process of sputter depositing the metal film on the surface of the substrate by using a sputter ion source: the ion beam sputtering energy of the sputtering ion source is 10-1000eV, the sputtering angle is 0-90 degrees, and the deposition angle is 10-90 degrees; the working pressure of the sputtering environment is 1.0 multiplied by 10 < -2 > to 5 multiplied by 10 < -2 > Pa, and the temperature of the substrate is 20 to 500 ℃.
optionally, in the process of sputtering and depositing the metal film on the surface of the substrate by using the sputtering ion source, the beam diameter of the sputtering ion source is 50-150 mm, the ion energy is 100-1000 eV, and the beam current density is 0.1-0.9 mA/cm 2; the beam diameter of the auxiliary ion source is 50-100mm, the ion energy is 200-700 eV, and the beam current density is 0.2-0.6 mA/cm 2.
Optionally, before the sputtering deposition of the metal film on the surface of the substrate by using the sputtering ion source, the method further comprises: and cleaning the surface of the substrate by ion beam bombardment by using the auxiliary ion source.
Optionally, the bombarding and cleaning the surface of the substrate comprises: and bombarding and cleaning the surface of the substrate for 1-20 min.
Optionally, before the sputtering deposition of the metal film on the surface of the substrate by using the sputtering ion source, the method further comprises: and drawing a vacuum to enable the substrate, the sputtering ion source and the auxiliary ion source to be positioned in a vacuum environment.
Optionally, the method further includes: and monitoring the thickness of the deposited metal film by using a crystal oscillator in the process of sputtering and depositing the metal film on the surface of the substrate by using a sputtering ion source.
in another aspect, a coater is provided, including:
A target platform;
A table, which can fix a substrate;
The sputtering ion source is used for bombarding the target platform and sputtering and depositing a metal film on the surface of the substrate through sputtering of the target platform;
and the auxiliary ion source is used for bombarding the metal film in the process of sputtering and depositing the metal film by the sputtering ion source so as to enhance the surface mobility of atoms of the metal film and improve the compactness of the metal film.
Optionally, in the process of sputter depositing a metal film on the surface of the substrate by using the sputter ion source: the ion beam sputtering energy of the sputtering ion source is 10-1000eV, the sputtering angle is 0-90 degrees, and the deposition angle is 10-90 degrees; the working pressure of the sputtering environment is 1.0 multiplied by 10 < -2 > to 5 multiplied by 10 < -2 > Pa, and the temperature of the substrate is 20 to 500 ℃.
Optionally, in the process of sputtering and depositing the metal film on the surface of the substrate by using the sputtering ion source, the beam diameter of the sputtering ion source is 50-150 mm, the ion energy is 100-1000 eV, and the beam current density is 0.1-0.9 mA/cm 2; the beam diameter of the auxiliary ion source is 50-100mm, the ion energy is 200-700 eV, and the beam current density is 0.2-0.6 mA/cm 2.
Optionally, the coating machine further includes: and the vacuum extraction module is used for extracting vacuum so that the substrate, the sputtering ion source and the auxiliary ion source are positioned in a vacuum environment.
Optionally, the coating machine further includes: and the crystal oscillator is used for monitoring the thickness of the metal film deposition.
One or more technical solutions provided in the embodiments of the present invention have at least the following technical effects or advantages:
1. According to the method and the coating machine provided by the embodiment of the application, in the process of sputtering the deposited metal film on the surface of the substrate by adopting the sputtering ion source, the metal film is bombarded by the auxiliary ion source, the surface mobility of the deposited metal atoms is enhanced by bombarding the surface layer of the growth film, the metal atom filling density is effectively improved, the metal film porosity is reduced, and the metal film density and the mechanical property under the condition of low-temperature film forming are enhanced. And by enhancing the surface mobility of metal atoms, the adhesive force between the metal film and the matrix is effectively improved, the aluminum film stress is obviously reduced, and the cracking problem caused by large internal stress is relieved, so that the metal film with high thickness and high density can be generated.
2. According to the method and the film coating machine provided by the embodiment of the application, before the sputtering ion source is adopted to sputter and deposit the metal film on the surface of the base body, the surface of the base body is bombarded and cleaned through the auxiliary ion source so as to remove impurities such as micro-dust, grease and the like on the surface of the base body, and the adhesive force between the metal film and the base body is improved. And the bombardment of the auxiliary ion source can activate the atoms on the surface of the base material, which is beneficial to depositing a compact metal film with more uniform crystal grains and smaller pores.
the foregoing description is only an overview of the technical solutions of the present invention, and the embodiments of the present invention are described below in order to make the technical means of the present invention more clearly understood and to make the above and other objects, features, and advantages of the present invention more clearly understandable.
drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and those skilled in the art can also obtain other drawings according to the drawings without creative efforts.
FIG. 1 is a diagram illustrating steps in a method for depositing a prepared film in an embodiment of the invention;
FIG. 2 is a graph showing the results of XRD tests in an example of the present invention;
FIG. 3 is an SEM image of a 5um thick aluminum film taken at 20 ten thousand times magnification in accordance with an embodiment of the present invention;
FIG. 4 is an SEM image of a 5um thick aluminum film magnified 50 ten thousand times in an embodiment of the present invention;
FIG. 5 is an SEM image of an aluminum film with a thickness of 10um magnified 20 ten thousand times in an embodiment of the present invention;
FIG. 6 is an SEM image of an aluminum film with a thickness of 10um magnified 50 ten thousand times in an embodiment of the present invention;
FIG. 7 is a schematic structural diagram of a coater according to an embodiment of the present invention;
FIG. 8 is a graph of RBS analysis results in an embodiment of the present invention.
Detailed Description
The embodiment of the application provides a method for preparing a film by deposition and a film coating machine, solves the technical problem that the existing metal film preparation scheme is difficult to prepare a metal film with both high thickness and high density, and provides a method for generating a metal film with high thickness and high density and a film coating machine.
The technical scheme in the embodiment of the application has the following general idea:
In the process of sputtering and depositing the metal film on the surface of the substrate by adopting a sputtering ion source, an auxiliary ion source is adopted to bombard the metal film so as to enhance the surface mobility of atoms of the metal film and improve the compactness of the metal film. Namely, the surface mobility of deposited metal atoms is enhanced through the auxiliary bombardment on the surface layer of the growing film, the filling density of the metal atoms is effectively improved, the void degree of the metal film is reduced, and the density and the mechanical property of the metal film under the condition of low-temperature film forming are enhanced. And by enhancing the surface mobility of metal atoms, the adhesive force between the metal film and the matrix is effectively improved, the aluminum film stress is obviously reduced, and the cracking problem caused by large internal stress is relieved, so that the metal film with high thickness and high density can be generated.
in addition, in order to realize good performance of the metal film, before the sputtering ion source is adopted to sputter and deposit the metal film on the surface of the base body, the surface of the base body is bombarded and cleaned by the auxiliary ion source so as to remove impurities such as micro-dust, grease and the like on the surface of the base body, and the adhesive force between the metal film and the base body is improved. And the bombardment of the auxiliary ion source can activate the atoms on the surface of the base material, which is beneficial to depositing a compact metal film with more uniform crystal grains and smaller pores.
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example one
In this embodiment, a method for depositing a prepared film is provided, as shown in fig. 1, the method comprising:
step S101, preparing a substrate;
and S102, sputtering and depositing a metal film on the surface of the substrate by using a sputtering ion source, wherein in the process of sputtering and depositing the metal film on the surface of the substrate by using the sputtering ion source, an auxiliary ion source is adopted to bombard the metal film so as to enhance the surface mobility of metal film atoms and improve the compactness of the metal film.
In the embodiment of the present application, the metal film may be an aluminum film, a copper film, a silver film, or a titanium film, which is not limited herein and is not listed.
Preferably, the metal film is an aluminum film, and the aluminum film has flat and high reflectivity from an ultraviolet region to an infrared region, and has good chemical stability due to the protection of a transparent Al2O3 film on the surface of the aluminum film. The absorption of the aluminum film is generally about 10%, that is, the reflectivity of the aluminum reflective film can reach about 90% at most, so the aluminum film is widely used as the reflective film of various reflective devices, and the demand for preparing the high-thickness and high-density aluminum film is high.
When the metal film is an aluminum film, preferably, the substrate is a fused silica material.
The detailed steps of the method for depositing and preparing the film provided by the application are described in detail below with reference to fig. 1:
First, step S101 is performed to prepare a substrate.
In the embodiment of the present application, the specific material of the substrate may be set according to specific needs, for example, the substrate may be an insulator such as glass, SiN or SiCO, a semiconductor such as silicon or germanium, or a conductor, which is not limited herein and is not listed.
in a specific implementation, the prepared substrate may be first mounted on a stage of a coater for depositing a metal film.
In the specific implementation process, after the substrate is fixed on a workbench of a coating machine, the coating machine performs vacuum extraction, so that the substrate, the sputtering ion source and the auxiliary ion source are positioned in a vacuum environment, and a clean vacuum deposition environment is provided for subsequent metal film deposition.
preferably, in this application embodiment, after preparing the base member, adopt the sputter ion source to be in through step S102 before the base member surface sputter deposition metal film, can also adopt auxiliary ion source earlier, through ion beam bombardment washing the base member surface, on the one hand, can clear away the impurity such as various micronic dust and grease on base member surface, improve the bonding strength of the metal film of follow-up preparation and base member, on the other hand, can make base member material surface atom activation through ion beam bombardment, be favorable to depositing the more even and compact metal film that the hole is littleer of crystalline grain.
Specifically, in order to achieve a better cleaning effect, when the auxiliary ion source is used for bombarding and cleaning the surface of the substrate, the time for bombarding and cleaning the surface of the substrate is 1-20 min, so that various impurities such as micro-dust, grease and the like on the surface of the substrate are thoroughly removed.
Preferably, in the embodiment of the present application, after the substrate is prepared, before the sputtering ion source is used to sputter deposit the metal film on the surface of the substrate in step S102, the target material of the target table may be cleaned by the sputtering ion source, so as to improve the purity of the metal film to be subsequently prepared. At the moment, the parameters of the sputtering ion source are set to be sputtering energy of 10-1000eV, and the time for sputtering and cleaning the target is 1-20 minutes.
next, step S102 is executed, and in the process of sputtering and depositing the metal film on the surface of the substrate by using the sputtering ion source, the metal film is bombarded by using the auxiliary ion source, so as to enhance the surface mobility of the metal film atoms and improve the compactness of the metal film.
In the embodiment of the application, before the sputtering ion source is adopted to sputter and deposit the metal film on the surface of the substrate, the parameters of the sputtering ion source and the auxiliary ion source are required to be set, the sputtering angle and the deposition angle are required to be adjusted, and the working air pressure and the substrate temperature of the film plating machine are required to be adjusted.
specifically, in the process of sputter depositing a metal film on the surface of the substrate using a sputter ion source, there may be provided:
The ion beam sputtering energy of the sputtering ion source is 10-1000eV, the sputtering angle is 0-90 degrees, and the deposition angle is 10-90 degrees; the beam diameter of the auxiliary ion source is 50-100mm, the ion energy is 100-700 eV, and the beam current density is 0.1-0.6 mA/cm 2; the working air pressure of the sputtering environment of the film coating machine is 1.0 multiplied by 10 < -2 > to 5 multiplied by 10 < -2 > Pa, and the temperature of the substrate is 20 to 500 degrees. The microstructure of the metal film in the film growth process such as grain size, preferred orientation, component proportion and the like can be controlled better through the setting of the parameters, and various physical and chemical properties of the film can be controlled effectively and flexibly.
Further, in order to increase the density of the deposited metal film, the parameter ratio of the sputtering ion source and the auxiliary ion source is optimally set in the embodiment of the application, and the following optimal parameter ranges are provided: during the process of sputtering and depositing the metal film on the surface of the substrate by adopting the sputtering ion source, the beam diameter of the sputtering ion source is 50-150 mm, the ion energy is 100-1000 eV, and the beam current density is 0.1-0.9 mA/cm 2; the beam diameter of the auxiliary ion source is 50-100mm, the ion energy is 200-700 eV, and the beam current density is 0.2-0.6 mA/cm 2. Through the arrangement of the sputtering and auxiliary optimal parameter ratio, the deposition quality of the metal film can be ensured, the surface mobility of deposited aluminum atoms can be enhanced more excellently, and the film-forming density and mechanical performance can be improved.
In the embodiment of the present application, according to different needs, different methods for bombarding the metal film by using different auxiliary ion sources during the process of sputter depositing the metal film by using a sputter ion source can be used, and three methods are listed as follows:
First, sputtering is performed while continuously performing auxiliary bombardment.
Namely, the auxiliary ion source is continuously started to bombard the metal film in deposition while the sputtering ion source is adopted to sputter and deposit the metal film, so that metal atoms in the sputtering and depositing process can be uniformly bombarded by the auxiliary ion source, thereby continuously keeping high mobility and improving the integral uniform density.
Second, the bombardment is intermittently assisted during sputtering.
That is, the auxiliary ion source is not continuously turned on for bombardment in the whole process of sputtering and depositing the metal film by the sputtering ion source, but is turned on intermittently as required to improve the surface mobility of the metal atoms.
For example, taking an aluminum film as an example, one of the reasons that it is difficult to form a thick film is that the aluminum film prepared by the existing process has poor bonding force with a substrate, has large internal stress and is easy to crack. Therefore, the auxiliary ion source can be started to bombard the metal film only at the initial stage of sputtering and depositing the metal film by adopting the sputtering ion source, so as to improve the bonding force between the metal film and the substrate.
Thirdly, the sputtering process is alternated with an auxiliary bombardment process.
Namely, during the process of sputtering and depositing the metal film by using a sputtering ion source, the bombardment of an auxiliary ion source is inserted. For example: the sputtering ion source can be started to perform metal film sputtering deposition to a preset thickness, then the sputtering ion source is closed, the auxiliary ion source is started to bombard the deposited metal film with the preset thickness, the surface mobility of the metal film is improved, then the auxiliary ion source is closed, the sputtering ion source is started to perform metal film deposition, and thus the sputtering deposition and the auxiliary bombardment are alternately performed according to a preset rule.
Of course, in the implementation process, in the process of sputter depositing the metal film by using the sputter ion source, the method of bombarding the metal film by the auxiliary ion source is not limited to the above three methods, and may be specifically set according to the requirement of the metal film to be deposited, and is not limited herein.
In a specific implementation process, in order to monitor the whole process of sputtering and depositing the metal film, a crystal oscillator can be used for monitoring the thickness of the metal film deposition in the process of sputtering and depositing the metal film on the surface of the substrate by using a sputtering ion source. Of course, an optical film thickness monitoring method may also be used to monitor the film thickness during the deposition of the metal film, which is not limited herein.
The metal film prepared by the method in the embodiment of the application has the advantages of high thickness and high density, and tests show that the density of the aluminum film prepared by the method in the embodiment of the application can reach 2.844g/cm3, and the grain size can reach 47.5nm due to the fact that the bulk density of aluminum is 2.7g/cm 3.
the following will illustrate the significant effects of the method for depositing a film provided in the embodiments of the present application, taking an aluminum film prepared on a fused silica wafer substrate by the method of the present embodiment as an example:
Firstly, by adopting the method provided by the embodiment of the application, the aluminum films with the film thicknesses of 5um and 10um are prepared on the fused quartz plate substrate, and the density of the aluminum film is calculated by adopting a weighing method, wherein the specific calculation method comprises the following steps:
After weighing, the mass of the fused quartz piece corresponding to the 5um aluminum film before film coating is 10.2488g, and the mass of the fused quartz piece corresponding to the 10um aluminum film is 10.2413 g. The mass of the fused quartz piece corresponding to the 5um aluminum film after film coating is 10.2716g, and the mass of the fused quartz piece corresponding to the 10um aluminum film is 10.2844 g. The mass of the 5 μm thick aluminum film was calculated to be 0.0228g and the mass of the 10 μm thick aluminum film was calculated to be 0.0431g by the subtraction. In combination with an aluminum film diameter of 45mm, it was calculated that a 5 μm thick aluminum film had a density of 2.844g/cm3, and a 10 μm thick aluminum film had a density of 2.798g/cm3, both greater than the bulk density of aluminum, 2.7g/cm 3.
It can be seen that the method provided by this example can be used to obtain a metal film with high thickness and high density.
To further illustrate the significant effect of the metal film prepared by the method of this embodiment, the aluminum film produced by the method provided by this embodiment is further subjected to an X-ray diffraction (X-ray diffraction) XRD test to detect the crystal orientation, peak position of diffraction peak, full width at half maximum of diffraction peak, and interplanar spacing of the produced aluminum film.
The detection results shown in fig. 2 and table 1 were obtained by XRD testing:
TABLE 1 aluminum film XRD test results
As can be seen from the test results in table 1 and fig. 2, the medium-thickness high-density aluminum film prepared by the method provided in this example has the following advantages over the aluminum film prepared by the conventional method:
the aluminum film prepared by the method of the embodiment only shows two diffraction peaks, namely (111) and (200). The diffraction peak position of the aluminum film (111) was 38.486 DEG, which is not much different from the standard peak position, and the amount of peak shift was extremely small. The diffraction peak position of the aluminum film (200) is 44.728 DEG, which is not much different from the standard peak position, and the amount of peak position shift is very small. The half widths of the diffraction peaks of the aluminum films (111) and (200) were 0.173 ° and 0.181 °, respectively, and the smaller the half width, the less the internal defects, the better the crystal orientation. Calculating the size of the aluminum crystal grains to be 47.5nm by adopting a Bragg equation according to the peak position and the full width at half maximum of the diffraction peak; the lattice strain calculated according to the peak position shift of different diffraction peaks and the corresponding change of the full width at half maximum is +0.0013, which shows that the residual internal stress in the sample is very small through the bombardment of the auxiliary ion source and meets the requirement.
to further illustrate the significant effect of the metal film prepared by the method of this embodiment, Scanning Electron Microscope (SEM) was also performed on the aluminum film generated by the method provided in this embodiment to determine whether there are a large number of voids and uniform distribution of crystals inside.
the results of the SEM examination are shown in fig. 3-6, wherein fig. 3 is a SEM image of the aluminum film with a thickness of 5um magnified by 20 ten thousand times, fig. 4 is a SEM image of the aluminum film with a thickness of 5um magnified by 50 ten thousand times, fig. 5 is a SEM image of the aluminum film with a thickness of 10um magnified by 20 ten thousand times, and fig. 6 is a SEM image of the aluminum film with a thickness of 10um magnified by 50 ten thousand times.
As can be seen from fig. 3 to 6, the 5um thick and 10um thick aluminum films prepared by the method provided by this embodiment have uniform grain size distribution, almost no voids, and good compactness.
To further illustrate the significant effect of the metal film prepared by the method of this embodiment, Rutherford Backscattering Spectrometry (RBS) analysis is also performed on the aluminum film generated by the method provided in this embodiment to detect the internal impurity elements and the content thereof.
The results of the measurement in FIG. 8 were obtained by RBS analysis, and as shown in FIG. 8, the impurity element in the resulting aluminum film was tungsten and the content thereof was less than 0.03 atmos%. According to the research, the influence of the tungsten impurity content on the mass density of the aluminum film is less than 0.004g/cm2, so that the aluminum film with the tungsten impurity content less than 0.03 atmos% is considered to be a high-density aluminum film.
therefore, the metal film prepared by the method provided by the embodiment can meet the requirements of preparing the metal film with high thickness and high compactness, and the prepared metal film has excellent quality indexes such as internal defects, crystal orientation, uniformity, impurity content, internal gaps and the like.
based on the same inventive concept, the application also provides a device corresponding to the method of the first embodiment, which is detailed in the second embodiment.
Example two
In this embodiment, as shown in fig. 7, there is provided a coater, including:
a target table 701;
A table 702, which can hold a substrate;
A sputtering ion source 703 for bombarding the target table, and sputtering and depositing a metal film on the surface of the substrate by sputtering of the target table;
And the auxiliary ion source 704 is used for bombarding the metal film in the process of sputtering and depositing the metal film by the sputtering ion source so as to enhance the surface mobility of atoms of the metal film and improve the compactness of the metal film.
As shown in fig. 7, the stage 702 corresponds to a position above the target stage 701, and in an implementation, the substrate may be fixed below the stage so that target atoms on the target stage 701 can be sputtered onto the substrate under bombardment by the sputter ion source 704. As also shown in FIG. 7, the bombardment direction of the auxiliary ion source faces the stage 702 so as to assist the bombardment on the surface of the substrate on the stage 702.
Further, the stage 702 is a rotary stage capable of changing the angle to adjust the position and angle of the substrate before sputtering the metal film.
In the embodiment of the application, in the process of sputtering and depositing the metal film on the surface of the substrate by using the sputtering ion source: the ion beam sputtering energy of the sputtering ion source is 10-1000eV, the sputtering angle is 0-90 degrees, and the deposition angle is 10-90 degrees; the beam diameter of the auxiliary ion source is 50-100mm, the ion energy is 100-700 eV, and the beam current density is 0.1-0.6 mA/cm 2; the working air pressure of the sputtering environment of the film coating machine is 1.0 multiplied by 10 < -2 > to 5 multiplied by 10 < -2 > Pa, and the temperature of the substrate is 20 to 500 ℃.
in the embodiment of the application, in the process of sputtering and depositing the metal film on the surface of the substrate by using the sputtering ion source, the beam diameter of the sputtering ion source is 50-150 mm, the ion energy is 100-1000 eV, and the beam current density is 0.1-0.9 mA/cm 2; the beam diameter of the auxiliary ion source is 50-100mm, the ion energy is 200-700 eV, and the beam current density is 0.2-0.6 mA/cm 2.
in this embodiment, the coating machine further includes:
And the vacuum extraction module is used for extracting vacuum so that the substrate, the sputtering ion source and the auxiliary ion source are positioned in a vacuum environment.
In this embodiment, the coating machine further includes: and the crystal oscillator is used for monitoring the thickness of the metal film deposition.
in order to further enhance the understanding of the embodiments of the present application, a specific deposition example is provided by combining the method of the first embodiment and the coater of the second embodiment to prepare an aluminum film on a fused silica wafer as an example:
First, a 2-inch fused quartz plate substrate is fixed below a workbench 702 shown in fig. 7, and a vacuum extraction module is started, so that the target stage 701, the workbench 702, the sputtering ion source 703 and the auxiliary ion source 704 are all in a vacuum environment;
Then, starting the auxiliary ion source 704 to bombard and clean the fused quartz plate for 1-20 minutes, and starting the sputtering ion source 703 to bombard and clean the target material on the target table 701 for 1-20 minutes;
next, adjusting parameters of the sputtering ion source and the auxiliary ion source, adjusting the sputtering angle and the deposition angle, and adjusting the working air pressure and the substrate temperature of the film plating machine according to the method provided by the first embodiment;
and then, starting the sputtering ion source and the auxiliary ion source to perform sputtering deposition of the metal film according to the method provided by the embodiment one, and monitoring the deposition thickness of the metal film through a crystal oscillator so as to stop deposition when the thickness requirement is met.
Since the film plating machine described in the second embodiment of the present invention is a device used for implementing the method for preparing a film by deposition according to the first embodiment of the present invention, a person skilled in the art can understand the specific structure and deformation of the device based on the method described in the first embodiment of the present invention, and thus the details thereof are not described herein. All the devices adopted in the method of the first embodiment of the present invention belong to the protection scope of the present invention.
The technical scheme provided in the embodiment of the application at least has the following technical effects or advantages:
1. according to the method and the coating machine provided by the embodiment of the application, in the process of sputtering the deposited metal film on the surface of the substrate by adopting the sputtering ion source, the metal film is bombarded by the auxiliary ion source, the surface mobility of the deposited metal atoms is enhanced by bombarding the surface layer of the growth film, the metal atom filling density is effectively improved, the metal film porosity is reduced, and the metal film density and the mechanical property under the condition of low-temperature film forming are enhanced. And by enhancing the surface mobility of metal atoms, the adhesive force between the metal film and the matrix is effectively improved, the aluminum film stress is obviously reduced, and the cracking problem caused by large internal stress is relieved, so that the metal film with high thickness and high density can be generated.
2. According to the method and the film coating machine provided by the embodiment of the application, before the sputtering ion source is adopted to sputter and deposit the metal film on the surface of the base body, the surface of the base body is bombarded and cleaned through the auxiliary ion source so as to remove impurities such as micro-dust, grease and the like on the surface of the base body, and the adhesive force between the metal film and the base body is improved. And the bombardment of the auxiliary ion source can activate the atoms on the surface of the base material, which is beneficial to depositing a compact metal film with more uniform crystal grains and smaller pores.
while preferred embodiments of the present invention have been described, additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. Therefore, it is intended that the appended claims be interpreted as including preferred embodiments and all such alterations and modifications as fall within the scope of the invention.
It will be apparent to those skilled in the art that various modifications and variations can be made in the embodiments of the present invention without departing from the spirit or scope of the embodiments of the invention. Thus, if such modifications and variations of the embodiments of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to encompass such modifications and variations.

Claims (13)

1. a method of depositing a prepared film, comprising:
preparing a substrate;
And sputtering and depositing a metal film on the surface of the substrate by adopting a sputtering ion source, wherein in the process of sputtering and depositing the metal film on the surface of the substrate by adopting the sputtering ion source, an auxiliary ion source is adopted to bombard the metal film so as to enhance the surface mobility of metal film atoms and improve the compactness of the metal film.
2. The method of claim 1, wherein the metal film is an aluminum film.
3. the method of claim 1, wherein during sputter deposition of the metal film on the substrate surface using a sputter ion source:
the ion beam sputtering energy of the sputtering ion source is 10-1000eV, the sputtering angle is 0-90 degrees, and the deposition angle is 10-90 degrees;
The working pressure of the sputtering environment is 1.0 multiplied by 10 < -2 > to 5 multiplied by 10 < -2 > Pa, and the temperature of the substrate is 20 to 500 ℃.
4. the method of claim 1, wherein during sputter deposition of a metal film on the substrate surface using the sputter ion source:
the beam diameter of the sputtering ion source is 50-150 mm, the ion energy is 100-1000 eV, and the beam current density is 0.1-0.9 mA/cm 2;
The beam diameter of the auxiliary ion source is 50-100mm, the ion energy is 200-700 eV, and the beam current density is 0.2-0.6 mA/cm 2.
5. the method of claim 1, further comprising, prior to said sputter depositing a metal film on said substrate surface using a sputter ion source:
And cleaning the surface of the substrate by ion beam bombardment by using the auxiliary ion source.
6. The method of claim 5, wherein said bombarding cleans said substrate surface, comprising:
And the time for bombarding and cleaning the surface of the substrate is 1-20 min.
7. The method of any of claims 1-6, further comprising, prior to the sputter depositing a metal film on the substrate surface using a sputter ion source:
and drawing a vacuum to enable the substrate, the sputtering ion source and the auxiliary ion source to be positioned in a vacuum environment.
8. The method of any of claims 1-6, further comprising:
and monitoring the thickness of the deposited metal film by using a crystal oscillator in the process of sputtering and depositing the metal film on the surface of the substrate by using a sputtering ion source.
9. A coating machine is characterized by comprising:
A target platform;
A table, which can fix a substrate;
the sputtering ion source is used for bombarding the target platform and sputtering and depositing a metal film on the surface of the substrate through sputtering of the target platform;
and the auxiliary ion source is used for bombarding the metal film in the process of sputtering and depositing the metal film by the sputtering ion source so as to enhance the surface mobility of atoms of the metal film and improve the compactness of the metal film.
10. the coater of claim 9 wherein during sputter deposition of a metal film on said substrate surface using said sputter ion source:
the ion beam sputtering energy of the sputtering ion source is 10-1000eV, the sputtering angle is 0-90 degrees, and the deposition angle is 10-90 degrees;
the working pressure of the sputtering environment is 1.0 multiplied by 10 < -2 > to 5 multiplied by 10 < -2 > Pa, and the temperature of the substrate is 20 to 500 ℃.
11. The coater of claim 9 wherein during sputter deposition of a metal film on said substrate surface using said sputter ion source:
The beam diameter of the sputtering ion source is 50-150 mm, the ion energy is 100-1000 eV, and the beam current density is 0.1-0.9 mA/cm 2;
The beam diameter of the auxiliary ion source is 50-100mm, the ion energy is 200-700 eV, and the beam current density is 0.2-0.6 mA/cm 2.
12. the coater of claim 9 further comprising:
And the vacuum extraction module is used for extracting vacuum so that the substrate, the sputtering ion source and the auxiliary ion source are positioned in a vacuum environment.
13. The coater of claim 9 further comprising:
And the crystal oscillator is used for monitoring the thickness of the metal film deposition.
CN201810525968.4A 2018-05-29 2018-05-29 Method for preparing film by deposition and film coating machine Pending CN110541153A (en)

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CN114855122A (en) * 2022-04-06 2022-08-05 湖南大学 Ultrathin metal film and preparation method and application thereof
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CN111812076A (en) * 2020-06-29 2020-10-23 河南科技大学 Flexible surface enhanced Raman effect substrate material and preparation method thereof
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CN116230843A (en) * 2022-12-29 2023-06-06 深圳惠科新材料股份有限公司 Manufacturing method of composite copper foil, composite copper foil and battery

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Application publication date: 20191206